Method for producing titanium compounds



Patented new, 1931' 1 i L17 1 32 710} noonn iiicri'owsxi, on 'GI'innnniini Clinton-i 'ro rITANrA CORPORA- j ron, 01F nos nivenr -nsoenrnon IA, AgjonRPoitn' rron on QALIEQRNIA} j mn'irnonro "zenonuenie ifi mnfrun qonleonnns 2*; c

The presentinventionreiatesespecialij ilt bo h 7' stablizing the interaction of-titaniumfnitro; reaotions,-=shown;bytheequations couldoccur 2' gen compounds and nitric acid with thegob ..si1nu1tanepus1y.;;; 3- Y P jectv ofpbtaining; new a and also more" uni- 1 Such considerations means 1 form products. 7 for controllingor; slowing-down 111161163 6: In my United StatesLette'rs'Patent Numtionsin s'uch away that amaximum yieldv of,

be'r 1,'7 t2,674, dated January 7, 1930, there-is" nitrogenconipounds mightbelf ormed togeth-.-'

described a inethodf or producing titanium: er;; Vit1ia;m1 'irnum amount of freeniti'ogen;

oxiderfronrtitanium nitrogen compounds by, As result-of those-studies I- have .now d1s no acting upo-nthem with n-nitric [acid-jfeither covegr edi t'hat ifsubstanees, he -added to the v aloneor in the presence of sulphuric acid reactants,r capablejofgivinginsolution ions wherehyonly abouta third of.;the;anitrogen 'ofphosphorusg compounds that these ions act of the titanium nitrogen compound; is; r e;j as; inhibitorsprnegat'iye catalysts andcause coverableintheformofan ammonium eome the nitric eid and titanium nitrogen: corn- 155 pound theremainder esoapingpresumahly nfpound to interact more slow-1y. Among the the form of g e s-Th f l wing? bs ancessuitablwi rt pu pQ men n, 1 equation illustrates that, reaction: soluble; p1iosp hates 11}phosphoric acid or,

be QXidiZ'Bd by. nitric acid to give phosphates;

.Y il he l d 3111 my pen mgtan e p p t hichundertheactioni 0i. Sui-1 I ve zphosphit sfior uch. mp u d ucan i Onem ye o us .c.on pou s su a cium t; 1 v

' cation [for Letters PatentI fieriall' -Number t' phuric ori otherfacidscan -forms0l11b1e;phos-' Q 320,762, iiiedflNoVemberQO, 1928 thatg r-nost "phat-lest;

.of the nitrogen oi the titaniumnitrogen g f[f, ghe f ,l'. id gamm f "-25. pounds is lost when one acts upon themwithl; trateibe allowedflto.interact witha titanium nitric acid in the presenceoif jsulphuric acidi nitrogen tcompound, or compounds; in the p '1 Inthis'instancethe object,ofjthe invention presenceef; water'iand sulphuric acid or a was the formation" oi new types o-fijfacld' halogen acid-For,mixtureaoisuehfacidsand:

titanium sulphates v he eb add -oui hese-z rea ts e m l 1301 It y h ef y fh ti t amou ofe; u tanceg pabl ;of.y n e or even more of the combined nitrogen of phosphate-iona smooth-reactionrtakes place the. titanium nitrogen compound, andby giving asvby-p'roducts'a uniform yield ofnititanium n1trogen,comp ound I mean titae-ii trogen compojundsg,.[lThis reaction therefore iIilulIl nitride or titan um cyanonitrlde' and gives ammoniumfc'ompounds,oftenassoc1at 1861' especially the reactive nitrogen compound d withjfgee' nitrog n and nitrogen o'xides,

prepared by the m thOdS my Un e jjStatesr together, with an. excellent yield-of a semc Letters Patent.;1,O8,61, dated Mar hjf; colloidal partly hydrated titanium oxide ofa p 1 922 could bereooteredfin a com bined' and: whiteer-vb-Luish white color having good cov 7 marketable form 'say as animonia or .a salt. ering power andpossessingia specificgravity 40; thereof, that s'uch,aibyeproduct wouldproye; lower, than that;of ianyuknown, titanium to'bequite ana's'setto thegabove mentioned? dioxide; j p p ces es- I di i a t9; mmQIliem 12 5 an: QX p e 0 he c y ng: u i' y pounds therei: also the possibility ofreco -e discover-X515:- lppl iedl-to the production 01$v 1 6 gf 16;O t -:c bi c knit oge y ne tani 1 1? de, lg v t ngs xq a n Will Show ne We he fih might tc fine' -th se pe. 9 my lwe nto this 1 happen: l Q examp l e zasonfiskiglled'intheartmay readilyf I, F Y; a ant m' i -f flN a2 gra n g f f 3 i1g form; of -oxides1ofnitrogen ThfiolloW-ing, pe imen bli t itiSitQbQ d at I d 595 There bfjcom the possihiiitj that other wenej'poure'd; into{ 40 cubic ricmsgi oflcold. water 109 phosphate.

and when the diluted acid was cool it was poured over 35 grams of commercial titanium cyanonitride contained in a 1500 cubic centimeter beaker. Next 35 grams of commercial sodium nitrate (chile saltpeter) were 7 dissolved in cubic cms.,of water and to this solution were "added 3 grams of sodium The aqueous solution of sodium nitrate and sodium phosphate was now poured into the. large beaker'containing the sulphuric "acid-titanium cyanonitride mixture. The materialswere stirred constantly and if necessary to start or accelerate the reaction they were warmed on the water bath. s v

The reaction went smoothly and after 24- hours no more reddishfcolored cyanonitride acid. The 'dioxide of titanium so obtained; was so finely divided that it passed through filter paper. Inorder to remove the last traces of acidremainingin the titanium oxidepa'ste it was neutralized with ammonia. It is evident that in place of using ammonia for thi'sneutralization that one could use other bases such as lime or barium hydrate oreven faintly basic or neutral substances such as barium'carbonate ort'he chlorides of barium or calcium or such other 'compounds'as would give volatile'acids upon drying.

'-After"the' pasty titanlum oxide had been thus neutralized with ammonia morewater wasadded. Next a few cubic centimeters of dilutehydrochloric acid were poured'in;

This acid was added to facilitatethe further washing of the oxide as the almost colloidal titanium dioxide settles out more rapidly from solutions containing halogen ions or having a definite hydrogen ionconcentration.

7 After one or two washings to remove any i11 t a ri aterialusually not quite as white but useammonium sulphate or other undesired substance the settled out hydrated titanium dioxide was evaporated to dryness.

There was thus obtained a white to bluish white hydrated titanium oxide containing, when drled at just below 100 cent., about 8% by weight of water. The dry powder had a specific gravity of 2.72; I

Such an oxide makes,when worked up in a suitable vehicle, an excellent pigment and because of its lowspecific gravity it does not settleout easily from liquid paints. The oxide ay be completely dehydrated by heatbelow a red heat and one thus obtains fulfor compounding with rubber or lino leum or for any other purpose forwhich titaniurn oxide is ordinarily'us'ed. 5,

. The working up oi the wash water for am monium compounds and the recovery of nitrogen oxides from the gases given off during the reaction follows well known practices.

It is obvious that when using different combinations' of reactants that different temperatures, pressures or concentrations may have to'be employed to obtain the desired results but these changes are well do not confine myself to such variations or tothe example as given but only to the claims.

What I claim as my invention is:

pounds which consists in stabilizing the interaction of nitric acid and titanium nitrogen compounds by carrying out the reactionin the presence of a phosphate ion.

2. Method for producing titanium compounds including titanium oxide of low specihc gravity whlch consists in stabilizing the interaction of nitric acid and titanium nitropresence of water by' acid as: an 1nh1b1tor.

gen compounds in the employing phosphoric v 3. Method for producing titanium compounds including titanium oxide of low specific gravity which consists in stabilizingthe; interactlon of nitric acid and titanium nitrogen compounds in the presence of water and sulphuric acid by employing alkali metal phosphate as an inhibitor. i

4. Method for producing titanium com-- pounds including titanium oxide of low specific gravity which consists in stabilizing the interaction of nitric acid which is generated in situ by sulphuric acid acting upon sodium nitrate and titanium nitrogen com" pounds while in the presence of water and sulphunc acid by employing alkali metal phosphate as an inhibitor.

' 5; Method for producing titanium compounds including titanium oxide of low specific gravity which consists in stabilizing the interaction of nitric acid which is generated in situ by sulphuric acid acting upon an alkali metal nitrate and titanium nitrogen'compounds while in the the presence of water and sulphuric acid by employing alkali metal phosphate as an inhibitor.

6. Method for producing titanium compounds including titanium oxide of low specific gravity whlch consists in stabilizing the interaction of nitric acid and titanium nitro gen compounds in the presence of sulphuric acid and water by employing calcium phosphate as an inhibitor.

7. Method for producing titanium oxideof low specific gravity which consists in stabilizingthe interaction of nitric acid and titanium nitrogen compounds in the presence of sulphuric acid ing a soluble phosphate as an inhibitor and recovering -semi-colloidal titanium oxide having a specific gravity less than 2.9;

- FOORD =.v'oN' BICHOWSKY.

within the scope. of studies made by one skilled inv the art. I

1.;Method for producing titanium comand water by employ 

